Method of making sulfur chlorid.



W. 0. QUAYLE. METHOD OF MAKING SULFUR GHLDRID.

APPLICATION FILED SEPT. 2, 1909 Patented June M, 1910.

M24966 as r I U I WILLIAM O. QUAYLE, OF WILMINGTON, DELAWARE, ASSIGNOR TO THE MIDLAND CHEMICAL COMPANY, OF MIDLAND, MICHIGAN, A CORPORATION OF IVIICHIGAN.

METHOD OF MAKING SULFUR CHLORID.

invention being herein explained and the best mode in which I have contemplated applying that principle, so as to distinguish it from other inventions.

The improved process herewith involved relates to the manufacture of sulfur chlorid (SCI and S Cl in general, but for the purpose of illustration such manufacture may be advantageously described as particularly related to the manufacture of carbon tetrachlorid. In such latter manufacture, the dichlorid is employed along with carbon disulfid, the chemical reaction involved be- QSOIZ+OSZ=C c is.

1 From the'resulting solution insuch manufacture of carbon tetrachlorid, the latter is distilled off leaving the sulfur resulting as per the above e nation in solution in the sulfur m nochlorid that is formed by the reaction 0 such sulfur with the excess of dichlorid employed in the reaction. The actual amount of sulfur thus carried in solution by the monochlorid is variable and for the purpose "ofwthisfl'rooe'ss is quite immaterial. The solution, owever,.is very readily formed. midat ordinary temperatures the chlorid may contain as much as per cent. of sulfur,' 'forniing a. thick -.syrupy' liquid. It is particularly with treatment of this residual solutionof the monochlorid and sulfur to produce more of the dichlorid for use over againinthe process just described that the present process is concerned, although as has been stated it obviously is a matter of indifference whether the resulting product be employed in the general. manufacturing o eration justdescribed or otherwise, or in eed, whether the sulfur be derived from a related process or be otherwise introduced. V

The object of this invention is to attain a more economicalutilization of the chlorin employed in chlorinating such sulfur and monochlorid and to prevent the escape of the readily volatile dichlorid into the atmos- Specification of Letters Patent.

Application filed September 2, 1909.

Patented June 14, 1910.

Serial No. 515,787.

phere, such escape being objectionable not merely because of the loss of the product thereby entailed, but also because of the highly objectionable odor of the compound in question.

To the accomplishment of these and re-.

lated objects the invention'consists of the steps hereinafter fully described and particularly set forth in the claims.

The annexed drawing and the following description set forth in detail one approved method of carrying out the invention, such disclosed'mode, however, constituting but one of various ways in which the principle of the invention may be used.

In said annexed drawing :-The single figure there appearing represents a part sectional view, more or less diagrammatic in character, of one approved type of apparatus for carrying out my process.

Having reference to the drawing, A will be seen to represent a reaction towerin the form of a closed, vertical, cylindrical chamber. The lower portion of the tower forms a tank a or storage base and above it is fixed a grating a upon which rests a quantity of suitable packing a such as coke. The upper portion of the tower is provided with a condenser a formed by water jacketed vapor tubes passing through tube sheets. A gas inlet pipe D enters below the grating and above the liquor level in the base, and a vapor outlet pipe C connects the upper portion of the tower above the condenser with a tower B similar to A, with the exception that it has no condenser and is provided with an exhaust fan G which draws gases.-

etc. from the upper portion of the tower and discharges through pipe 9. Two storage tanks F and H are placed above, the former of which drains into the tower A by means of the valved pipes, as shown; while a pump E, connected with the towers by valved pipes e, is adapted to draw liquor from the bases of said towers and lift it to either tank F or H, as desired, through another valved pipe 6 In the utilization of the above described apparatus for the manufacture of sulfur chlorids by my improved process, liquid sulfur monochlorid containing sulfur in solution, as before described, is supplied to the tank F and is allowed to run from it by way of the pipe 'f into the tower A, where it trickles down over the coke or other pack rest upon the packing b and I find that l which it trickles, an

ing employed, finally dripping into the storage base below. Thence such liquid is drawn and returned by the pump E into the tank F, or if desired it may be diverted into tank H. Simultaneously with the passage of this stream of sulfur chlorid in one direction through the reaction tower A, a gaseous body admitted through the inlet pipe D is drawn upwardly :through the tower A, thence through the connecting pipe 0. and in like manner upwardly through the tower B, be-

ing finally discharged by the exhaust fan G through the pipe 9. Such gaseous body consists of chlorin which should be dry but which may be diluted with air, as is usual in commercial'practice. Owing to the heat generated by the reaction in tower A between chlorin and the monochlorid or sulfur, part of the dichlorid formed-is vola tilized and is carried forward with theunabsorbed air or other inert gases present. It is the office of the condenser a to cool, condense and return the larger part of this vapor to the tower v acking below it, 0m

d finally drips into the storage base. The uncondensed dichlorid vapor and unabsorbed chlorin passes out of the upper portion of tower A with the inert gases and are drawn upwardly through the secondtower B. In order to retain this chlorin and dichlorid, the tower B is charged with a quantity of sulfur b in pieces which -pumped by pump E into the tank F. It

will be seen, therefore, that by my improved process the' eater part of the sulfur used is introduce pipes in the liquid, dissolved, form without opening the reaction chambers or towers, and that the small amount of solid sulfur required to be charged is introduced at the ,tinlctlg into the apparatus through exhaust end of the system where the presence of vapor and odor is least, and in fact, prac tically negli 'ble. I secure thereby the most complete uti ization of the chlorin and sulfur withthe least incidental loss and nuisance, and the control of the process is rendered easier and more simple than in any other process with which I am acquainted.

Other modes of applying the principle of my invention may be employed instead of the one explained, change being made as regards the process herein disclosed, provided the step or steps stated by any one of the following claims or the equivalents of such stated ste or steps be employed.

I there ore particularly point out and disclaim as m invent1on: n the manu acture of sulfur chlorids, thesteps which consist in chlorinating sulfur in solution, and absorbing any escaping chlorin or chlorid Vapors with solid sulfur.

2. In the manufacture of sulfur dichlorid, the steps which consist inv chlorinating sulfur in solution to such dichlorid, and absorbing any escaping chlorin or dichlorid vapors with solid sulfur.

3. In the manufacture of sulfur dichlorid, the steps which consist in chlorinating a solution of sulfur mono-chlorid and sulfur, and absorbing any escapingchlorin or dichlorid vapors with solid sulfur.

4:. In the manufacture of sulfur dichlorid, the steps which consist in passing a gaseous body containing chlorin through a solution of sulfur mono-chlorid and sulfur, whereby sulfur dichlorid is produced, and then passing the residual gases, including any unabsorbed chlorin or vaporized dichlorid, over solid sulfur, whereby such chlorin and dichlorid vapors are absorbed.

5. The improvement in the manufacture of sulfur chlorids, which consists in absorbing in solid sulfur any chlorin or chlorid vapors that escape from the principal reactions.

Signed by me'this 28th day 'of August, 1909.

' WILLIAM O. QUAYLE. Attested by OLENA DONALD, Lrzzm COCHRAN. 

